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以水合三氯化铱和 dfppy 为原料,在乙二醇单乙醚溶剂中反应得氯桥二聚体(dfppy)2Ir(μ-Cl2)Ir(dfppy)2,然后在碱性条件下与2-吡啶甲酸反应合成出 FIrpic。通过核磁共振谱(1HNMR、13CNMR)、质谱、红外光谱和单晶X射线衍射等确定了分子结构,高效液相色谱法(HPLC)测试了纯度,利用紫外-可见吸收光谱和光致发光光谱对其光物理性能进行了测试。结果表明:FIrpic为电中性八面体配合物,在476 nm处出现了较强的蓝光发射,其合成产率大于90%,纯度为99.22%,该方法适于FIrpic的批量制备。

A new chemical technique was developed for batch synthesis of bis(4,6-difluorophenyl-pyridine)(picolinate)iridium(III), an organometallic light-emitting molecule for OLED. The process involves cycometalation of IrCl3·nH2O with 2-(2,4-difluorophenyl)pyridine and cleavage of chloride-bridged dimer by 2-pyridinecarboxylic acid to produce the desired compound in a 20~30 gram batch scale. The yield was more than 90%, and the purity was determined by HPLC to be 99.22%. The chemical structure of bis(4,6-difluorophenyl-pyridine)(picolinate)iridium(III) was verified by NMR (1H and 13C), MS and FT-IR along with single crystal X-ray diffraction data. The synthesized FIrpic is an electrically neutral octahedral complex. A strong blue-emission at 476 nm was observed in ultraviolet-visible and photoluminescence absorption spectra of the compound.

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